CN104120287B - Technique for enriching and recovering indium and associated copper from low-concentration indium-containing solution - Google Patents
Technique for enriching and recovering indium and associated copper from low-concentration indium-containing solution Download PDFInfo
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- CN104120287B CN104120287B CN201410302226.7A CN201410302226A CN104120287B CN 104120287 B CN104120287 B CN 104120287B CN 201410302226 A CN201410302226 A CN 201410302226A CN 104120287 B CN104120287 B CN 104120287B
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Abstract
The invention relates to a technique for enriching and recovering indium and associated copper from a low-concentration indium-containing solution. The low-concentration indium-containing solution is a zinc oxide low immersion liquid which mainly contains 200-300 mg/L In<3+>, 100-150 g/L Zn<2+>, 10-30 g/L H2SO4, trace-3.5 g/L Cu<2+>, 5-15 g/L total Fe, trace-8 g/L Fe<3+> and 0.8-2.5 As <3+>. The technique comprises the following steps: adding a copper-containing solution into the low-concentration indium-containing solution to obtain a mixed solution, wherein the copper-containing solution is a lead zinc smelting production solution and mainly contains 5-35 g/L Cu<2+>, trace-10 g/L Cd<2+>, 25-35 g/L H2SO4 and 5-10 g/L Fe<3+>; adding zinc scum into the mixed solution to carry out neutralization reaction, wherein the zinc scum is mainly composed of 75-85% of ZnO, 15-25% of Zn gold, 0.8-4.5% of Cl and 1-2% of S; and controlling the pH value of the neutralization reaction end point at 4-6, hydrolyzing until the pH value is 6.5, carrying out liquid-solid separation to obtain a filtration residue and a filtrate after the reaction finishes, leaching the filtration residue in acid to obtain an indium-rich solution, and extracting to obtain the metal indium, wherein the copper residue is used as a copper smelting raw material. By using the waste zinc scum as the neutralization reducer and manually changing the indium/copper proportion of the solution, the indium enters in the form of In(OH)3 residues, thereby lowering the residue quantity and creating favorable conditions for subsequent indium extraction while enriching the indium.
Description
Technical field
The invention belongs to a kind of hydrometallurgical technology, specifically refer to a kind of technique containing enriching and reclaiming indium and association copper solution of indium from lower concentration.
Background technology
Occurring in nature seldom has the Independent Mineral of indium, but is present in other mineral with low content of accompanying form, is more common in Pb-Zn deposits.So the many by products from lead-zinc smelting of extraction raw material of indium or waste, these wastes come in every shape, complicated component, and indium content is extremely low.But indium is a kind of rare precious metal, industrial purposes is also relatively more extensive, although the extraction of indium is very difficult, really very valuable.
In industry, from lower concentration waste liquid, the method for Enrichment Indium, copper mainly contains hydrolysis method, oxidation-reduction method, extraction process etc., adopts which kind of technology or method, depends on mineral resources or SOLUTION PROPERTIES.Indium is carried containing the burnett's solution of indium for lower concentration, main employing reduction adds extraction process, the problem of the method is that extraction process emulsification is more serious, production to be started shooting difficulty, and extraction quantity is large, the organism that raffinate is carried secretly enters Zn system in a large number and causes zinc electrolysis to burn plate, and wherein reason is many-sided, but a large amount of Zn
2+, Fe
3+, Cu
2+, Mn
2+isoionic existence is one of the main reasons.Can how to remove this interfering ion be in advance the precondition avoiding these phenomenons to occur.
In lead-zinc smelting, in byproduct, in waste, synthetical recovery association copper is wherein related to a Business Economic Benefit.Association copper reclaims mainly with wet processing, but in practice, the leaching process of copper invariably accompanies while the impurity such as a large amount of iron, silicon, cadmium and leaches, and how to reclaim association copper in conjunction with the indium recovery process in low concentration solution be that people wish to solve and one of important topic of not resolving for a long time simultaneously.
Summary of the invention
Object of the present invention is exactly propose that a kind of the lower concentration that this technique can effectively produce from the systems such as electric zinc, containing Enrichment Indium in solution of indium, reclaims copper simultaneously from the technique of lower concentration containing enriching and reclaiming indium solution of indium and association copper, a large amount of Zn when avoiding follow-up indium extraction operation
2+, Fe
3+, Cu
2+, Mn
2+plasma disturbs, and improves work efficiency and comprehensive utilization of resources level.
This technique containing enriching and reclaiming indium and association copper solution of indium from lower concentration that the present invention proposes, is characterized in that:
(1) lower concentration is the low immersion liquid of zinc oxide containing solution of indium, and it is mainly containing In
3+: 200-300mg/l, Zn
2+: 100-150g/l, H
2sO
4: 10-30g/l, Cu
2+: trace-3.5g/l, Fe
entirely: 5-15g/l, Fe
3+: trace-8g/l, As
3+: 0.8-2.5g/l;
(2) lower concentration adds copper-containing solution obtain mixed solution containing solution of indium, and this copper-containing solution is the solution of lead-zinc smelting output, and it is mainly containing Cu
2+: 5 ~ 35g/l, Cd
2+: trace ~ 10g/l, H
2sO
4: 25 ~ 35g/l, Fe
3+: 5 ~ 10 g/l;
(3) add neutralizing agent zinc dross in mixed solution and carry out neutralization reaction, zinc dross main component is ZnO:75 ~ 85%, Zn
gold: 15 ~ 25%, Cl:0.8 ~ 4.5%, S:1 ~ 2%; H wherein
2sO
4neutralized by ZnO, pH value constantly rises; Cu
2+by Zn
golddisplacement, enters in slag with the form of copper sponge, Fe
3+major part is by Zn
goldbe reduced into Fe
2+; In
3+there is hydrolysis reaction, with In(OH)
3in form slag input;
(4) pH value of neutralization reaction terminal controls at 4-6, hydrolysis pH value 6.5, and reaction end is carried out solid-liquor separation and obtained filter residue and filtrate, and filtrate send iron removal step process, and filter residue, will with In(OH through one section of low acid and one section of high acidic oils)
3the indium that form exists immerses solution again, and copper is stayed in slag, and solid-liquor separation obtains rich solution of indium and copper ashes, and rich solution of indium treatment by extraction obtains indium metal, and copper ashes is then as copper metallurgy raw material.
Zinc dross is levigate powder, and granularity is-200 order ~ 6 orders.Powder can increase with by the contact area of reactant, improve speed of response and reaction mass.
Above-mentioned operation (3) neutralization is fractional neutralization selective cementation with displacement operation: first 1
#react in groove, control temperature is at 80-90 DEG C, and pH value is 0.5 ~ 2.0, in reaction process while consumption acid, and Zn
goldmain and Cu
2+, Fe
3+reaction, and Zn all in raw material in this groove
goldconsume completely, avoid In
3+be reduced to simple substance In; 2
#groove temperature controls at 80-90 DEG C, continues to add zinc dross and carries out neutralization reaction, and it is 3.5 ~ 4.0 that pH value controls, most In
3+with In(OH in this groove)
3form slag input; 3
#groove temperature controls more than 85 DEG C, under naturally stirring, make pH value reach 5.0, reduces the condition that toxic and harmful hydrogen arsenide produces further, realizes safety in production.
In above-mentioned operation (4), the temperature of filter residue one section of Weak-acid leaching controls at 80 ~ 90 DEG C, and terminal acidity is 50 ~ 70g/l, more than 12 hours reaction times, and institute's acid adding is 98% vitriol oil, and adjusting slurry is for producing water, and leach liquor is containing In
3+: 2.5 ~ 3.5g/l, Zn
2+: 30 ~ 80 g/l, Cu
2+: trace, Fe
3+≤ 1.0g/l.The filtrate of Weak-acid leaching operation is rich solution of indium.
In above-mentioned operation (4), one section of high acidic oils is that temperature controls at 80 ~ 90 DEG C by Weak-acid leaching gained filter residue high acidic oils, and terminal acidity is 150 ~ 180g/l, more than 12 hours reaction times, institute's acid adding is 98% vitriol oil, and adjusting slurry is for producing water, and leach liquor is containing In
3+: 0.3 ~ 1g/l, Zn
2+: 30 ~ 60g/l, Cu
2+: trace, Fe
3+≤ 1.0g/l.
The filtrate of high acidic oils returns Weak-acid leaching operation and continues to participate in reaction, and filter residue is made for copper metallurgy raw material.
" Zn of the present invention
gold" be expressed as the zinc of metallic state, " trace " represents that certain constituent concentration is not equal to zero close to zero, similarly, " Fe
entirely" represent full iron.
Add in zinc dross and in the operation of displacement at above-mentioned mixed solution, there is following chemical reaction:
In
3++ Zn→In↓+ Zn
2+………… ①
Cu
2++Zn→Cu↓+ Zn
2+………………②
Fe
3++Zn→Fe
2++ Zn
2+……………… ③
1. this reaction is that the present invention does not wish to see because the bad leaching of indium metal precipitated with substitute mode, utilize just 2. simultaneously, 3. two reactions the metallic zinc in zinc dross is run out of.Along with the carrying out of neutralization reaction, thus make most of In
3+there is following reaction:
In
3++3OH
-→In（OH）
3↓………………④
4. reaction is that the present invention wishes to see, because In(OH)
3chance acid and solubilized enter in solution with ionic condition, and good leaching, can reach the object of the first step enrichment.2. the bad leaching of the metallic copper in, also stays in slag after meeting acid, thus achieves indium, measuring copper and separation respectively.
From said process, how to control reaction conditions, allow metallic zinc preferential substitution cupric ion and high price iron, avoid as far as possible zinc replace indium ion be the key that can obtain high indium recovery.
The present invention utilize the waste zinc dross of by-product in zinc metallurgy as in and reductive agent, people for a change lower concentration, containing the indium copper proportionlity of solution of indium, replaces, allows indium with the In(OH easily leached with making zinc metal selective)
3form slag input, this mode changing slag type artificially greatly reduces the quantity of slag, makes slag contain indium and reaches 10000g/t, cupric more than 10%, while effective Enrichment Indium metal, for follow-up indium extraction creates favourable condition.Therefore, the present invention be in fact one from the new way of lower concentration containing enriching and reclaiming indium solution of indium.
Accompanying drawing explanation
Accompanying drawing is process flow diagram of the present invention.
Embodiment
Positively effect of the present invention is further illustrated below with example.
Example 1
A collection of lower concentration contains In containing solution of indium
3+202mg/l, Zn
2+100g/l, H
2sO
410g/l, Cu
2+trace, Fe
entirely5g/l, Fe
3+4g/l, As
3+1.0g/l.Copper-containing solution is containing Cu
2+: 35g/l, Cd
2+: 2g/l, H
2sO
4: 25g/l, Fe
3+: 5 g/l.Two kinds of solution by volume 1:0.1 ratio is mixed to get mixed solution.
Neutralizing agent zinc dross used is containing ZnO:80%, Zn
gold: 15%, Cl:0.8%; S:2%, granularity is-200 orders.Obtain mixed solution in 1:0.1 ratio as calculated, be incorporated into contained Zn in the total amount of the zinc dross needed for neutralization reaction
goldinsufficient total amount with Cu
2+, Fe
3+there is replacement(metathesis)reaction completely, also need supplement add a certain amount of zinc powder, 250kg about per hour.
Through technical process as shown in the figure and above-mentioned steps process, gained indium copper segregation slag is containing indium 15320g/t, and cupric 17.5% indium copper segregation slag obtains rich solution of indium containing In through one section of Weak-acid leaching
3+2.58g/l, the indium concentration ratio containing solution of indium relative to original lower concentration is 12.8 times, and the rate of recovery is 98.6%.
The gained copper ashes cupric 51% after high acidic oils operation process of a leached mud after Weak-acid leaching.Return that to change rate be 97.2% relative to original copper-containing solution.
Example 2
Another batch of lower concentration contains In containing solution of indium
3+: 260mg/l, Zn
2+: 120g/l, H
2sO
4: 20g/l, Cu
2+: 2 g/l, Fe
entirely:
10g/l, Fe
3+: 1g/l, As
3+: 2.0g/l.Copper-containing solution is containing Cu
2+: 20g/l, Cd
2+: 2g/l, H
2sO
4: 30g/l, Fe
3+: 8 g/l.Two kinds of solution by volume 1:0.2 ratio is mixed to get mixed solution.
Neutralizing agent zinc dross used is containing ZnO:75%, Zn
gold: 20%, Cl:1.8%; S:1%, granularity is-200 orders.Obtain mixed solution in 1:0.2 ratio as calculated, be incorporated into contained Zn in the total amount of the zinc dross needed for neutralization reaction
goldinsufficient total amount with Cu
2+, Fe
3+there is replacement(metathesis)reaction completely, also need supplement add a certain amount of zinc powder, 80kg about per hour.
The technological process of process is same as Example 1.Acquired results is as follows:
Indium copper segregation slag is containing indium 18340g/t, and cupric 13.8% indium copper segregation slag obtains rich solution of indium containing In through one section of Weak-acid leaching
3+3.31g/l, the indium concentration ratio containing solution of indium relative to original lower concentration is 12.7 times, and the rate of recovery is 98.2%.
The gained copper ashes cupric 47% after high acidic oils operation process of a leached mud after Weak-acid leaching.Be 96% relative to the rate of recovery of original copper-containing solution.
Example 3
Another batch of lower concentration contains In containing solution of indium
3+: 300mg/l, Zn
2+: 150g/l, H
2sO
4: 30g/l, Cu
2+: 3.5 g/l, Fe
entirely:
15g/l, Fe
3+: 8g/l, As
3+: 2.5g/l.Copper-containing solution is containing Cu
2+: 35g/l, Cd
2+: 10g/l, H
2sO
4: 35g/l, Fe
3+: 10 g/l.Two kinds of solution by volume 1:0.3 ratio is mixed to get mixed solution.
Neutralizing agent zinc dross used is containing ZnO:85%, Zn
gold: 25%, Cl:4.3%; S:2%, granularity is-200 orders.Obtain mixed solution in 1:0.3 ratio as calculated, be incorporated into contained Zn in the total amount of the zinc dross needed for neutralization reaction
goldinsufficient total amount with Cu
2+, Fe
3+there is replacement(metathesis)reaction completely, also need supplement add a certain amount of zinc powder, 450kg about per hour.
The technological process of process is same as Example 1.Acquired results is as follows:
Indium copper segregation slag is containing indium 23220g/t, and cupric 23% indium copper segregation slag obtains rich solution of indium containing In through one section of Weak-acid leaching
3+3.57g/l, the indium concentration ratio containing solution of indium relative to original lower concentration is 11.9 times, and the rate of recovery is 98.7%.
The gained copper ashes cupric 53% after high acidic oils operation process of a leached mud after Weak-acid leaching.Be 97.2% relative to the rate of recovery of original copper-containing solution.
Claims (6)
1. contain a technique for enriching and reclaiming indium and association copper solution of indium from lower concentration, it is characterized in that:
(1) lower concentration is the low immersion liquid of zinc oxide containing solution of indium, and it is mainly containing In
3+: 200-300mg/l, Zn
2+: 100-150g/l, H
2sO
4: 10-30g/l, Cu
2+: trace-3.5g/l, Fe
entirely: 5-15g/l, Fe
3+: trace-8g/l, As
3+: 0.8-2.5g/l;
(2) lower concentration adds copper-containing solution obtain mixed solution containing solution of indium, and this copper-containing solution is the solution of lead-zinc smelting output, and it is mainly containing Cu
2+: 5 ~ 35g/l, Cd
2+: trace ~ 10g/l, H
2sO
4: 25 ~ 35g/l, Fe
3+: 5 ~ 10 g/l;
(3) add neutralizing agent zinc dross in mixed solution and carry out neutralization reaction, zinc dross main component is ZnO:75 ~ 85%, Zn
gold: 15 ~ 25%, Cl:0.8 ~ 4.5%, S:1 ~ 2%; H wherein
2sO
4neutralized by ZnO, pH value constantly rises; Cu
2+by Zn
golddisplacement, enters in slag with the form of copper sponge, Fe
3+major part is by Zn
goldbe reduced into Fe
2+; In
3+there is hydrolysis reaction, with In(OH)
3in form slag input;
(4) pH value of neutralization reaction terminal controls at 4-6, hydrolysis pH value 6.5, and reaction end is carried out solid-liquor separation and obtained filter residue and filtrate, and filtrate send iron removal step process, and filter residue, will with In(OH through one section of low acid and one section of high acidic oils)
3the indium that form exists immerses solution again, and copper is stayed in slag, and solid-liquor separation obtains rich solution of indium and copper ashes, and rich solution of indium treatment by extraction obtains indium metal, and copper ashes is then as copper metallurgy raw material.
2. contain the technique of enriching and reclaiming indium and association copper solution of indium as claimed in claim 1 from lower concentration, it is characterized in that zinc dross is levigate powder, granularity is-200 order ~ 6 orders.
3. contain the technique of enriching and reclaiming indium and association copper solution of indium as claimed in claim 1 from lower concentration, it is characterized in that operation (3) neutralization is fractional neutralization selective cementation with displacement operation: first 1
#react in groove, control temperature is at 80-90 DEG C, and pH value is 0.5 ~ 2.0, in reaction process while consumption acid, and Zn
goldmain and Cu
2+, Fe
3+reaction, and Zn all in raw material in this groove
goldconsume completely, avoid In
3+be reduced to simple substance In; 2
#groove temperature controls at 80-90 DEG C, continues to add zinc dross and carries out neutralization reaction, and it is 3.5 ~ 4.0 that pH value controls, most In
3+with In(OH in this groove)
3form slag input; 3
#groove temperature controls more than 85 DEG C, under naturally stirring, make pH value reach 5.0, reduces the condition that toxic and harmful hydrogen arsenide produces further, realizes safety in production.
4. the technique of enriching and reclaiming indium and association copper solution of indium is contained as claimed in claim 1 from lower concentration, it is characterized in that the temperature of filter residue one section of Weak-acid leaching in operation (4) controls at 80 ~ 90 DEG C, terminal acidity is 50 ~ 70g/l, more than 12 hours reaction times, institute's acid adding is 98% vitriol oil, adjusting slurry is for producing water, and leach liquor is containing In
3+: 2.5 ~ 3.5g/l, Zn
2+: 30 ~ 80 g/l, Cu
2+: trace, Fe
3+≤ 1.0g/l, the filtrate of Weak-acid leaching operation is rich solution of indium.
5. the technique of enriching and reclaiming indium and association copper solution of indium is contained as claimed in claim 1 from lower concentration, it is characterized in that in above-mentioned operation (4), one section of high acidic oils is by Weak-acid leaching gained filter residue high acidic oils, temperature controls at 80 ~ 90 DEG C, terminal acidity is 150 ~ 180g/l, more than 12 hours reaction times, institute's acid adding is 98% vitriol oil, and adjusting slurry is for producing water, and leach liquor is containing In
3+: 0.3 ~ 1g/l, Zn
2+: 30 ~ 60g/l, Cu
2+: trace, Fe
3+≤ 1.0g/l.
6. as described in one of claim 1-5, contain the technique of enriching and reclaiming indium and association copper solution of indium from lower concentration, it is characterized in that the filtrate of high acidic oils returns Weak-acid leaching operation and continues to participate in reaction, filter residue is made for copper metallurgy raw material.
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|---|---|---|---|
| CN201410302226.7A CN104120287B (en) | 2014-06-30 | 2014-06-30 | Technique for enriching and recovering indium and associated copper from low-concentration indium-containing solution |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410302226.7A CN104120287B (en) | 2014-06-30 | 2014-06-30 | Technique for enriching and recovering indium and associated copper from low-concentration indium-containing solution |
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| CN104120287B true CN104120287B (en) | 2015-06-24 |
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| CN108486365B (en) * | 2018-02-01 | 2019-10-25 | 云南云铜锌业股份有限公司 | A method of the Enrichment Indium from the low material of zinc abstraction containing indium |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3976743A (en) * | 1974-09-13 | 1976-08-24 | Cominco Ltd. | Treatment of zinc plant residue |
| CN101994009A (en) * | 2010-12-10 | 2011-03-30 | 株洲冶炼集团股份有限公司 | Method for enriching and recovering indium from zinc oxide acid supernate |
| CN102560147A (en) * | 2011-12-30 | 2012-07-11 | 株洲冶炼集团股份有限公司 | Method for recovering zinc from indium raffinate and zinc scum |
-
2014
- 2014-06-30 CN CN201410302226.7A patent/CN104120287B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3976743A (en) * | 1974-09-13 | 1976-08-24 | Cominco Ltd. | Treatment of zinc plant residue |
| CN101994009A (en) * | 2010-12-10 | 2011-03-30 | 株洲冶炼集团股份有限公司 | Method for enriching and recovering indium from zinc oxide acid supernate |
| CN102560147A (en) * | 2011-12-30 | 2012-07-11 | 株洲冶炼集团股份有限公司 | Method for recovering zinc from indium raffinate and zinc scum |
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